Review of the fundamentals of thin-film growth

Norbert Kaiser

The properties of a thin film of a given material depend on the films real structure. The real structure
is defined as the link between a thin films deposition parameters and its properties. To facilitate
engineering the properties of a thin film by manipulating its real structure, thin-film formation is
reviewed as a process starting with nucleation followed by coalescence and subsequent thickness growth,
all stages of which can be influenced by deposition parameters. The focus in this review is on dielectric
and metallic films and their optical properties. In contrast to optoelectronics all these film growth
possibilities for the engineering of novel optical films with extraordinary properties are just beginning to
be used. 2002 Optical Society of America
OCIS codes: 310.0310, 310.1620, 310.1860, 310.3840, 310.6860, 310.6870.

1. Introduction

The dependence of optical properties on deposition

conditions is a severe constraint in reproducing thin
films performance. There is a significant conflict
between performance models based on ideal- and
real-structure films. Models are required that relate real-film structure to desired optical properties.
This knowledge would permit the design and manufacture of coatings based on more-realistic production
conditions than are now possible. In this review aspects of thin-film growth in various dimensions, from
isolated nanoclusters to continuous macroscopic
films, are treated. The focus is on dielectric and
metallic films and their optical properties.
Investigations of process parameters, real structures, and film properties have been in progress for
many years, starting in 1938 with the classic research of Hass.1 Perusal of Refs. 27 is recommended as an introduction to the structure-related
optical properties of thin films.
2. Real Structure

The ideal structure of solids is either ideally ordered

single-crystalline or ideally disordered amorphous.
But there is no ideal crystalline or amorphous structure in the real world. The real structure of single
crystals always has a certain number of intrinsic and

N. Kaiser kaiser@iof.fhg.de is with the Fraunhofer Institute of

Applied Optics and Precision Engineering, Schillerstrasse 1, 07741
Jena, Germany.
Received 14 August 2001.
0003-693502163053-08$15.000
2002 Optical Society of America

extrinsic defects. Intrinsic defects are those that are

caused by atoms not changing the stoichiometry of
the crystal. Defects that produce nonstoichiometry
are called extrinsic defects. Defects generally can
have a major influence on the physical properties of
the solid, for instance, on the transmission of light
and on electrical conductivity.
The growth of thin films by physical-vapor deposition is an extremely nonequilibrium process that
takes place at high supersaturations and at comparatively high concentrations of impurity atoms. Consequently the number of extrinsic and intrinsic
defects in thin films may exceed that in bulk solids by
5 orders of magnitude. As a result of the usual
deposition conditions in optics and of the surface
structure of optical components, optical films are generally polycrystalline. This means that the real film
consists of defect-rich crystalline grains, which are
separated by impurity-enriched grain boundaries.
This is the reason why film properties differ significantly from bulk properties. Figure 1 shows this
fact schematically. The real structure of thin films
is a metastable nonequilibrium state that is far away
from its energetic minimum. Real structure tends
to change whenever enough energy is available.
Real structure is the link between thin-film deposition parameters and thin-film properties Fig. 2.
In engineering electronic and optical properties it is
vital to control stoichiometry, mean grain size, and
grain size distribution of the thin-film structure.
For engineering of film properties through real structure, models are indispensable. In what follows,
thin-film formation is described as a kinetic adsorption and diffusion process starting with nucleation,
coalescence, and subsequent thickness growth,
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3053

Fig. 4. Initial states of film growth after Ref. 9. , substrate

surface coverage in monolayers ML.

Fig. 1. Left, ideal single-crystalline substrate coated with ideal

single-crystalline films. Incoming light with intensity I0 is split
into reflected and transmitted parts IR and IT, respectively. Conservation of energy is given by I0 IR IT. Right, real substrate
with real coatings. Part of incoming intensity I0 is absorbed IA
or scattered IS. Conservation of energy is given by I0 IR
I T IA I S .

whereby all states can be influenced by deposition

parameters.
3. Growth of Thin Films
A.

Nucleation

The production of thin films by vapor deposition is a

classic case of heterogeneous nucleation, i.e., the condensation of adatoms at a substrate that is composed

Fig. 2. Factors that control the properties of thin films.

of atoms that are different from those of the vapor.

Figure 3 shows the various stages of thin-film growth.
Nucleation takes place at high supersaturations S,
defined as
S pp e,

(1)

where p is the vapor pressure of the deposit material

evaporated from the source at temperature T and po
is the equilibrium vapor pressure of the substrate
material at temperature TS. Deposition rate R is
related to p as
R p2mKT 12,

(2)

K is Boltzmanns constant, m is the molecular weight

of the deposit material, and T is the temperature of
the evaporation source. Because S is extremely
high, S 1051050 S 4 in a Wilson chamber,
nucleation is a nonequilibrium process, which can
best be described by the mean-field nucleation theory.8
As for all phase transitions, the formation of thin
films is characterized by the formation of nuclei and
their growth. Depending on the interaction energies of substrate atoms and film atoms, any of three
growth modes Fig. 4 can occur:

Fig. 3. TEM micrographs of antimony film formation nucleation, growth of nuclei, coalescence, channels, holes, homogeneous film.
Here as is special for Sb at percolation an amorphous crystalline phase transition change of contrast takes place.
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APPLIED OPTICS Vol. 41, No. 16 1 June 2002

trons through the network and conductivity rises

steeply by several orders of magnitude. Obviously,
a phase transition takes place at the percolation
threshold, with optical film properties changing exponentially. It is shown that this phenomenon is
crucial when it comes to engineering thin semitransparent metal films.
Fig. 5. Wetting angle of a liquid nucleus on a substrate is
described by Youngs equation: B * A cos , where B is
the surface energy of substrate, A is the surface energy of film
material, and * is the interface energy filmsubstrate.

Layer by Layer In the two-dimensional

Frankvan der Merwe mode, layers of material grow
one on top of another. Interaction between substrate and film atoms is greater than between adjacent film atoms.
Island In the VolmerWeber mode, separate
three-dimensional islands form on the substrate.
Interaction between film atoms is greater than between adjacent film and substrate atoms.
Layer plus Island In the StranskiKrastanov
mode, one or two monolayers form first, followed by
individual islands.

Growth modes can be systematically classified in

terms of surface energies with Youngs equation
taken into account Fig. 5.
Island growth 0 requires that B A *,
whereas layer growth 0 requires that B A
*. Layer-plus-island growth occurs because the interface energy increases with film thickness; typically
the layer on top of the substrate is strained to fit the
substrate. The growth mode is controlled not only
by interface energies but also by supersaturation.10
Generally, growth tends to shift from island to layer
as supersaturation increases.
B.

Coalescence

The next stage of three-dimensional film formation is

the growth of islands until they touch one another to
form a continuous network. This so-called coalescence process is extremely important for the design of
films with special properties. After solidlike coalescence of two islands there may remain a grain boundary between them, or they may fuse together in a
liquidlike fashion to form a new, larger, and
boundary-free island. Surface energies and supersaturation are the factors that control these processes
through material transport by surface and bulk diffusion. The transition from isolated islands to a continuous macroscopic network can be characterized by
a percolation threshold thickness. To percolate
means to pass or to cause to pass through a porous
material. This definition can be understood, for example, from measurements of electrical conductivity
between two macroscopically separated contacts
upon an insulating substrate during the growth of a
metallic layer between them. At percolation thickness, coalescence creates a continuous path for elec-

C.

Thickness Growth

The mean percolation thickness for many films is

120 nm. The thickness required for producing
metal mirror layers or dielectric quarter-wave systems is, however, larger than that value. Further
material deposition does not simply increase thickness; moreover, the real structure is determined by
the following four processes:
Shadowing A geometric interaction between
the arriving admolecules and the roughness of the
growing surface. This effect is dominant at low substrate temperatures TS. It occurs because the vapor
beam is directed.
Surface diffusion Mobility of admolecules at
surfaces and interfaces such as grain boundaries;
dominant at medium substrate temperatures TS.
Bulk diffusion Mobility of admolecules in the
volume of grains; dominant at high TS.
Recrystallization Phase transition as a complete change of crystal orientation; dominant at percolation thickness, large film thickness, and high TS.

For most metals and dielectrics, activation energies

for diffusion are related to the melting temperature of
the material, Tm. Thus different basic processes can
be expected to dominate different ranges of TsTm
and to determine the real structure. This is the concept of so-called structure zone models.11 In the
simplest case, real structure exists in three zones:
Zone I TsTm 0.3 low mobility; admolecules
stick where they land; the result is a fine-grained
porous real structure.
Zone II 0.3 TsTm 0.5 surface diffusion
occurs with activation energies of 0.1 0.3 eV; a columnar real structure is obtained.
Zone III TsTm 0.5 bulk diffusion occurs
with activation energies above 0.3 eV, resulting in a
rough equiaxed grained real structure.

Such a generalization of homologous structure

zone models in terms of physical processes is important for engineering film properties. Structure zone
models have been deduced by Thornton for sputtered
films1215 and by Messier et al.16 and Messier17 for
ion-assisted deposition. Additionally, Grovenor et
al.18 take the influence of substrate morphology into
consideration. For comparison, all models mentioned are shown in Fig. 6.
Until now it has only briefly been mentioned that
the growth of thin films for optics by physical-vapor
deposition is a comparatively dirty process. Indeed,
under high-vacuum conditions in a normal produc1 June 2002 Vol. 41, No. 16 APPLIED OPTICS

3055

Fig. 6. Structure zone models after Movchan,11 Thornton,12 Messier et al.,16 and Grovenor et al.18.

tion environment the rate of residual gas molecules

water, hydrocarbons, etc. striking the substrate surface is of the same order of magnitude as the deposition rate of the film material. At a total pressure of
104 Pa it takes only 1 s to form one monolayer of
residual gas molecules upon the substrate. Consequently, extrinsic impurity defects, whether present
on the substrate surface or resulting from the evaporation source or from the residual gas, have a great
influence on film growth. The effect is comparable
with that of the substrate temperature. Impurities
markedly change the surface energies at all stages of
film growth. Impurities that are not soluble in the
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APPLIED OPTICS Vol. 41, No. 16 1 June 2002

lattice are segregated into the grain boundaries and

onto the growing film surface. At a critical impurity
concentration, a fixed passivation layer forms, upon
which secondary nucleation may occur. Therefore,
nondiluted impurities are concentrated at interfaces.
In real structures, large impurity concentrations
act in the same way as low substrate temperatures.
Structure zones are shifted along the TsTm axis toward a fine crystalline, porous structure. Barnal
and Adamik19 introduced the basic structure zone
model, which starts from the basic case of impurityfree films Fig. 7 and then takes the increasing influence of impurities into consideration.

Table 1. Rate of Absorption Values to Defect Concentration in

Dielectric Thin Films

Type of Film

ND cm3

cm1

k250 nm

Single crystal
Thin film
Basic absorption

1013
1018
1022

103
102
106

10 m
100 m
10 nm

2 109
2 104
2

Absorption cross section for one photon is approximated by the area of one atom 1016 cm2.23 Table
1 lists typical defect concentrations ND, absorption
coefficients , optical penetration depths 1, and
extinction coefficients k250nm at 250-nm wavelength. The photon absorption cross section was estimated to be 1016 cm2. Basic absorption means
absorption for wavelengths below the shortwave absorption edge.
Furthermore, real structure causes scatter losses.
All types of real-structure phenomena such as grains,
pores, defects, and rough interfaces are directly connected to scattering.24
5. Metal Films

Fig. 7. Basic and real-structure zone models for low, medium, and
high impurity concentrations after Barna19.

4. Dielectric Films

Classic optical interference film systems are now applied down to the vacuum-ultraviolet excimer-laser
wavelength range. Here the individual quarterwave fluoride films can be as thin as 10 nm. Structure zone models Figs. 6 and 7 show the real
structure of dielectric thin films. The connection between optical properties and real structure is possible
by effective medium theories on the basis of the classic LorenzLorentz model, e.g., for TiO2.20 Optical
effects are inhomogeneities and anisotropies, i.e.,
complex refractive-index changes with variable film
thickness and angle of incidence of light. Optical
anisotropies caused by columnar film growth can be
used for special applications, such as polarizers for
normal incidence.21,22 This application is the most
prominent example of how to make a virtue of necessity and how a microstructure can be tailored by
means of growth phenomena.
Optical absorption is caused by defects hosted in
the porous film structure. In most cases these defects are water, oxygen, and hydrocarbons. As mentioned above, thin films contain higher numbers of
defects, by 5 orders of magnitude, than do bulk
materials. To estimate how a concentration ND of
absorbing defects per volume unit influences absorption coefficient , one can use the simple relation
N D.

(3)

Growth of metal films starts with islands the

VolmerWeber mechanism. Island films are transparent to visible and infrared radiation. At percolation thickness the film becomes continuous and is
transparent in the visible spectral region while it
reflects the infrared. Finally, at larger thicknesses
all radiation is reflected. This process is one of the
most exciting phenomena in optics: Properties
change with film real structure only by addition of
some nanometers of metal material, as is shown schematically in Fig. 8.
A.

Metal Island Films

As has been known for many years, metal island films

Ag, Au, Cu, . . . do not behave optically similarly to
the corresponding bulk material.25 Fifty years ago
this effect was called Anomalien der optischen Konstanten anomalies of optical constants. Today
these properties are of outstanding importance in optics.26 Metal islands may interact with light over
surface plasmons, namely, by agency of plasmon
polaritons. Plasmons are strong collective oscillations of electrons in the island in phase with the
incoming light. The Mie resonance frequency of the
oscillation depends on three factors: the electronic

Fig. 8. Growth of a metal film, starting from islands to continuous

transparent to nontransparent films.
1 June 2002 Vol. 41, No. 16 APPLIED OPTICS

3057

properties of the metal, the size and shape of the

islands, and the properties of host material in which
the islands are embedded or upon whose surface they
are fixed.
Because metals are highly absorbing, only small
changes in cluster size and distribution can be used to
engineer the optical properties of the ensemble. Optical constants can be calculated on the basis of
MaxwellGarnett models and of the Drude theory of
free electrons.27,28 Practical applications of island
films require a macroscopic matrix in which the sensitive nanometer-sized metal clusters are embedded.
In an optical film design, metal islands can be embedded in barrier layers such as SiOx, Al2O3, and
NiCr to prevent oxidation or in other matrices such as
transparent conductive oxides. Metal island films
have become important elements of present-day optics and optoelectronics. Intensive research is being
conducted into active optoelectronic elements that
consist of island films, including optically active individual molecules. As an example of optically active molecules, the StranskiKrastanov layer-plusisland growth of Ge islands upon Si substrates for the
production of self-assembled quantum dots may be
mentioned.29 Such deposition can be performed
only under ultrahigh vacuum conditions and upon
clean single crystalline surfaces. In optics, deposition conditions are far from being so well defined.
However, there are many industrial applications that
make use of the optical, electronic, and mechanical
properties of metal island films. Classic examples of
nano-optics are the red and yellow colors of Middle
Ages church windows, photographic systems, and solar absorbers. Recent applications in the field of
photonic bandgap materials are based on ultrafast
light-switching phenomena, which can by used as
novel components in integrated optics for biosensors or optical tweezers. We are just beginning to
use them in the engineering of novel optical films
with extraordinary properties.
B.

Continuous Transparent Metal Films

At thicknesses greater than the percolation thickness, metal films behave optically similarly to the
corresponding bulk materials and are transparent to
visible radiation and reflective for infrared radiation
as long as the thickness is less than 20 nm. In this
thickness interval, transparent metal films can be
used as neutral beam splitters, induced transmission
filters, solar control coatings, thermal insulating
coatings, transparent electrodes, and heating layers.
For example, silver is used for neutral-color highly
transparent and thermal insulation coatings low
emissivity, variably colored solar control coatings,
and low-emissivity Sun coatings.30,31 For reduction
of absorption, the percolation thickness should be as
low as possible. Maximum wetting of the substrate
can be achieved in the two-dimensional Frankvan
der Merwe growth mode. Unfortunately, as was already mentioned, optical film growth starts with
three-dimensional islands. In that case one can decrease the percolation thickness by increasing the
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APPLIED OPTICS Vol. 41, No. 16 1 June 2002

Fig. 9. Cross-sectional transmission electron microscopy picture

of CrSc multilayer mirrors with period spacing d 1.57 nm left
and d 3.17 nm right.34

number of islands per unit area. At the same mean

film thickness, many small islands cover a larger
substrate area than do fewer but large islands. Tailoring percolation thickness to minimum values by
increasing the deposition rate and reducing the substrate temperature is not possible, owing to the severe technological restrictions that are typical for
large-area architectural coatings. However, the
concept of changing surface energies Fig. 5 can be
applied successfully. This can be done by plasma
pretreatment of the substrate or by use of ultrathin
bonding layers such as Cr, Pd, and NiCr. Also, ion
assistance can be used.32 At larger thicknesses,
however, abnormal grain growth occurs,33 as predicted by Grovenors structure zone model18 Fig. 6.
Wetting can also be improved by the use of such
semiconductive transparent oxides as In2O3, SnO2,
ZnO2, and In2O3 doped with 210% Sn. These oxides are frequently used instead of, or mixtured with,
metals. Finding the best engineering technology is
currently a field of keen competition among largearea coaters. State-of-the-art basic knowledge of
film growth is of hardly any help today for finding
solutions to improve wetting.
Another application of continuous metal films is as
multilayer mirror coatings for soft x radiation especially in the water window: 2.3 4.4 nm and for
extreme-ultraviolet radiation 10 100 nm. Important applications in this context are microlithography, x-ray astronomy, plasma spectroscopy, medical
engineering, x-ray microscopy on live tissue, and laser research and synchrotron radiation research.34
What has been achieved is near-picometer precision
for the production of nanometer multilayer mirrors
for x rays Fig. 9. With ultraprecise biased magnetron sputtering it takes only approximately an hour
to deposit 600 layers for that wavelength range.35
C.

Continuous Nontransparent Metal Films

Continuous nontransparent metal films have long

been used as mirrors. It has been shown that, at
high deposition rates and low substrate temperatures, nucleation density is high and that consequently thin films have a fine polycrystalline

microstructure and maximum reflectivity. This has

been known for many years by industrial producers of
metal mirrors as the quick-and-cold rule.

6. Summary

The growth of optical thin films starts with adsorption and diffusion of individual atoms. The structure
of polished optical surfaces is rather less well-defined
in terms of surface energy and can be characterized
only by integral values. The maximum permissible
substrate temperature in optics is 300 C, and deposition rates are in the ranges of some nanometers
per second. At the same rate, foreign atoms from
the residual gas impinge upon the substrate surface.
Therefore nucleation starts statistically with the formation of three-dimensional islands VolmerWeber
mechanism. Next, coalescence leads to a macroscopic network, and at percolation thickness the optical and also all other properties change abruptly.
Further thickness growth leads often to a polycrystalline real structure. Films consist of grains that
range from a few nanometers to several micrometers
in size. Grain boundary regions can have volume
fractions comparable with those of the grains. Consequently the properties of thin films differ markedly
from the bulk properties of the same material.
Thin-film properties are directly related to the films
real structure. The study of structureproperty relationships is therefore indispensable for engineering
thin films. Substrate temperature and deposition
rate can be varied only within a limited range. Film
growth can be influenced more effectively by changes
of the substrate surface energy and an increase in the
energy of adatoms.
Substrate surfaces can be pretreated with different
kinds of plasmas and ions and by prenucleation with
subnanometer bonding islands. The energy of adatoms can be increased by all types of energetic deposition, especially by use of ion assistance. Where
applicable, sputter technology leads to much more
defined film properties, because the energy of adatoms is in the region of some electron volts, compared
to only 0.1 eV with electron-beam or boat evaporation. Film growth in optics in contrast to in electronics is rather undefined and poorly understood.
Despite the fact that optical coatings are used with an
ever-increasing leverage effect on optics, we are only
just beginning to understand film growth in detail.
Film growth is a unique low-cost nanofabrication process. It has the property of self-assembling material
over large areas into periodic structures that exhibit
photonic bandgap properties. For controlling the
optical properties of films nowadays it is of utmost
importance to have a thorough knowledge of real
structure on an atomic scale.
The author thanks Hans Pulker for fruitful discussions and critical inspection of the manuscript and
Ute Kaiser for preparing the cross-sectional transmission electron microscopy picture of the CrSc multilayer mirror.

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